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EP2004880A2 - Procédé de réalisation d'une électrode en diamant et électrode en diamant - Google Patents

Procédé de réalisation d'une électrode en diamant et électrode en diamant

Info

Publication number
EP2004880A2
EP2004880A2 EP07727806A EP07727806A EP2004880A2 EP 2004880 A2 EP2004880 A2 EP 2004880A2 EP 07727806 A EP07727806 A EP 07727806A EP 07727806 A EP07727806 A EP 07727806A EP 2004880 A2 EP2004880 A2 EP 2004880A2
Authority
EP
European Patent Office
Prior art keywords
diamond
layer
carrier layer
diamond electrode
diamond particles
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP07727806A
Other languages
German (de)
English (en)
Other versions
EP2004880B1 (fr
EP2004880B8 (fr
Inventor
Michael Schelch
Wolfgang Staber
Wolfgang Wesner
Robert Hermann
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Pro Aqua Diamantelektroden Produktion GmbH and Co KG
Original Assignee
Pro Aqua Diamantelektroden Produktion GmbH and Co KG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Pro Aqua Diamantelektroden Produktion GmbH and Co KG filed Critical Pro Aqua Diamantelektroden Produktion GmbH and Co KG
Publication of EP2004880A2 publication Critical patent/EP2004880A2/fr
Publication of EP2004880B1 publication Critical patent/EP2004880B1/fr
Application granted granted Critical
Publication of EP2004880B8 publication Critical patent/EP2004880B8/fr
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2264/00—Composition or properties of particles which form a particulate layer or are present as additives
    • B32B2264/10—Inorganic particles
    • B32B2264/107—Ceramic
    • B32B2264/108—Carbon, e.g. graphite particles
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C02F2001/46133—Electrodes characterised by the material
    • C02F2001/46138—Electrodes comprising a substrate and a coating
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/49826—Assembling or joining
    • Y10T29/49908—Joining by deforming

Definitions

  • the invention relates to a method for producing a diamond electrode with synthetically produced and electrically conductive (doped) diamond particles, which are embedded in a carrier layer.
  • the invention further relates to a diamond electrode with synthetically produced and electrically conductive (doped) diamond particles embedded in a carrier layer.
  • Diamond electrodes are characterized by a high overvoltage for oxygen and hydrogen and are therefore particularly suitable for a variety of oxidation processes in aqueous solution. Possible and particularly interesting applications are in the field of water treatment by anodic oxidation and in the field of synthetic chemistry.
  • Diamond particles are mixed with powders of metals or metal alloys which are capable of forming a non-conductive oxide layer, and then pressed, so that a pressing part, possibly with a carrier plate, is formed, which embedded the diamond particles in one or more layers contains.
  • low-melting materials for example magnesium or a magnesium alloy, are proposed, which are melted onto a preferably metallic support layer having a higher melting point.
  • WO 2005/16298 deals with the production of plastic diamond electrodes
  • JP 2005272908 of which a bipolar diamond electrode is known
  • US 2005200260 which relates to a method in which Metal is deposited on diamonds.
  • Diamond electrodes made by the named CVD method are limited in size. Larger electrode surfaces tend to crack due to the different thermal expansion coefficients, which can subsequently lead to destruction of the electrode by gas evolution under the diamond layer.
  • the diamond layer must therefore, to ensure the durability of the electrode, have a certain minimum thickness, which can only be achieved by a multi-hour deposition process. The production costs are therefore comparatively high in the case of diamond electrodes produced in this way.
  • Diamond electrodes which are produced according to EP 1527212 by the attachment of diamond particles to self-passivating metals, have a good durability in those media in which the metal oxide is stable under anodic or cathodic conditions. In strongly halide-containing aqueous solutions and in organic solutions, such as those used in electro-organic synthesis, the durability of such electrodes is somewhat lower. In AC applications, hydride corrosion affects the durability of the electrodes.
  • the invention has for its object to provide a process for the preparation of well-tolerated in aggressive media diamond electrodes and corresponding diamond electrodes.
  • Diamond electrodes produced according to the invention are intended, in particular, in halogen acids, in salt solutions, sols, Seawater and in the organic synthesis with alcoholates particularly durable.
  • the object is achieved according to the invention characterized in that the doped diamond particles are introduced in one layer between two films forming the carrier layer, wherein the films are then firmly bonded together and the diamond particles are exposed on both sides of the carrier layer.
  • Diamond electrodes designed according to the invention are characterized in that the diamond particles are embedded in one layer in the carrier layer and are exposed on both sides of the carrier layer.
  • Diamond electrodes produced and embodied according to the invention can be obtained by selecting the film material in the aforementioned aggressive media, such as
  • Halogen acids, salt solutions, brine and seawater as well as in the organic synthesis with alcoholates be very durable. Their range of application extends over the entire pH range from 0 to 14. Diamond electrodes according to the invention are also largely maintenance-free, since by reversal of deposits, such as lime, can be resolved so that does not need to be washed with acid. Diamond electrodes produced and embodied according to the invention can furthermore be used as anode or as cathode, they can be reversed regularly or operated with alternating current without the electrodes being damaged by hydride formation.
  • the material used for the carrier layer, for the mechanical fixation of the diamond particles, glass, ceramic, or a plastic in particular Teflon, PVDF, PFA, PTFE, FEP, ETFE, PEEK or PPS, used (claims 2 and 8 ). These materials are equally well suited under cathodic and anodic conditions and show no sensitivity to hydride corrosion, oxygen corrosion or other chemical agents.
  • the films, between which the doped diamond particles are introduced have a thickness of 5 ⁇ m to 300 ⁇ m, preferably a thickness of 10 ⁇ m to 150 ⁇ m (claim 8). To connect the two films are, for example, heating (over Schmelztempertaur), welding, soldering, sintering, pressing, rolling or gluing (claim 3).
  • a support grid, support fabric or the like between the two films is introduced to increase the mechanical strength, before they are firmly joined together (claim 9).
  • the grid or the fabric even after the completion of the diamond electrode by conventional methods of connecting plastics with plastics or metals, for example by lamination or gluing one or both sides are fixed to the surface of the diamond electrode (claim 10).
  • Support fabrics or support grids are plastics, such as Teflon, PVDF, PFA, PTFE, FEP, ETFE, PEEK or PPS, glass fibers, plastic-coated glass fibers, ceramics or metals, such as titanium or tantalum, used (claim 1 1).
  • the diamond particles are already exposed in the step of heating (melting).
  • an additional, soft material in the form of thin plates is placed on the outside of the carrier layer-forming films, into which the diamond particles penetrate by applying two-sided or one-sided pressure and are therefore exposed (claim 4).
  • a material for these plates are, for example, Teflon, Viton, Kapton, neoprene, thermoplastic vulcanizates (TPV), fluoropolymers such as PO, fluororubbers such. FPM or FKM, PEEK, silicones but also metals, such as e.g. Lead, aluminum or copper, in question (claim 5).
  • the thickness of these materials is 0.2 mm to 3 mm, in a preferred embodiment 0.5 mm to 1, 5 mm (claim 6).
  • the diamond particles on both sides of the support layer for example on mechanical, chemical or thermal manner, exposed (claim 7). In this way it can be ensured in each case that the diamond particles can be contacted on both sides of the carrier layer.
  • a contacting layer can be applied on one side, which permanently enables the diamond particles to be supplied with current (claim 13).
  • electrically conductive material are mainly graphite, carbon or carbon fibers in question. This material may be a powder, a paste or a fabric (claims 14 and 15).
  • a conductive salt solution preferably Na 2 SO 4 , can be used to improve the contact (claim 16).
  • FIG. 1 shows schematically a cross section through an inventively designed and manufactured diamond electrode.
  • the diamond electrode shown in the drawing figure consists of a layer of diamond particles 2 which are embedded in a carrier layer 1.
  • Diamond particles 2 are embedded in one layer without mutual contact with each other in the carrier layer 1 in such a way that they protrude slightly from both sides of the carrier layer 1 and are exposed.
  • a contacting layer 3 made of an electrically conductive material is applied on the one side of the carrier layer 1. Through the contacting layer 3, the power supply 4 takes place.
  • diamond particles 2 of very different shape and size and from different production processes can be used.
  • Particularly suitable conductive or semiconducting diamond powder which has a particle size of 80 .mu.m to 500 .mu.m, in particular up to 300 microns.
  • Diamond particles 2 are doped in particular with boron or nitrogen.
  • a preferred starting material for the preparation of diamond electrodes according to the invention are doped boron dopants produced by the high-pressure high-temperature process Industrial diamonds, which have a particularly high proportion of sp3 carbon.
  • the carrier layer 1 is used for mechanical fixation of the diamond particles 2, in particular in a plane, and consists of one in each
  • inert material which is preferably insensitive to hydride corrosion, oxygen corrosion and other chemical agents
  • glass, ceramic and chemically stable polymers such as fluorinated polymers such as Teflon, PVDF, PFA, PTFE, FEP, ETFE, PEEK or PPS.
  • the starting material for the carrier layer 1 are preferably films.
  • the diamond particles 2 between two sheets of the selected material, such as glass, ceramic or plastic, embedded. Subsequently, the two films are joined together, for example by heating (melting), welding, soldering, sintering, pressing, rolling or gluing.
  • the films have a thickness of 5 .mu.m to 300 .mu.m, preferably from 10 .mu.m to 150 .mu.m. If necessary, the raised portions of the diamond particles are exposed on both sides, for example, in a mechanical, chemical or thermal manner.
  • a soft material in the form of thin plates is placed on the outer sides of the films forming the carrier layer.
  • TPV thermoplastic vulcanizates
  • fluoropolymers such as PO
  • fluororubbers such as FPM or FKM
  • PEEK thermoplastic vulcanizates
  • the thickness of the plates is chosen between 0.2 mm to 3 mm, in particular between 0.5 mm and 1, 5 mm. If necessary, a complete exposure of the diamond particles can also take place in a mechanical or chemical or thermal manner in a further processing step.
  • a supporting grid, supporting fabric or the like can be introduced between the two films during the production of the diamond electrode. However, it is also possible, a support grid, supporting fabric or the like after the completion of
  • plastics or metals in question for example, lamination or gluing.
  • Suitable materials for the support grid, supporting fabric or the like are plastics such as Teflon, PVDF, PFA, PTFE, FEP, ETFE, PEEK or PPF, glass fibers, plastic-coated glass fibers, ceramics or metals, such as titanium or tantalum.
  • a contacting layer 3 can be attached, which makes it possible to permanently supply the diamond particles 2 with electricity.
  • all types of conductive materials are suitable for the contacting layer 3.
  • a durable and liquid-tight integration of the diamond particles 2 in the carrier layer 1 is hardly possible. It can not be ruled out that diamond particles 2 lose the connection to the carrier layer 1 in some places during operation of the electrode.
  • the processes that can cause a detachment are not only of a chemical nature, such as oxidation and corrosion, but also have physical causes. For example, heat generation by current flow can lead to cracking between the diamond particles 2 and the carrier layer material.
  • the evolution of gas on the anodic or cathodic diamond electrode can cause strong forces, which cause a slow weakening of the connection. After a certain period of operation, although the diamond particles 2 are still in their position, but it is possible that liquid penetrates to the contacting layer 3.
  • the contacting layer 3 In order to ensure a very long shelf life even in aggressive media, it is therefore important to carry out the contacting layer 3 such that, in spite of penetrating liquid and possible corrosion of the material of the contacting layer 3, a permanent contact with the diamond particles 2 is ensured.
  • Halogen acids and alcoholates under anodic conditions separate as material for the contacting layer 3 virtually all metallic conductors.
  • the contacting layer 3 either conductive materials, for example ceramics or plastics, or materials which do not form insulating oxides, for example graphite, carbon or carbon fibers, are used.
  • conductive carbon forms such as graphite, carbon or carbon fibers. While these materials oxidize upon contact with the solution under anodic potential, they only release carbon dioxide, which escapes through the material, which is more porous as it is present as a bed of particles or powder, as a paste or tissue. The material contracts and ensures constant contact with the diamond particles. A certain removal of carbon is accepted, which is compensated by a corresponding supply of material of the contacting layer. The total amount of electricity which is directly converted via the contacting (electrolysis) can be neglected in relation to that supplied to the diamond particles 2.
  • drainage of the contacting layer 3 can be provided, whereby penetrating solution on the contacting layer 3 can be actively removed. This can preferably take place by means of the gas pressure, which arises as a result of the electrolysis in the contact space, via suitable openings 4.
  • the contacting layer 3 may additionally be filled with a conducting salt solution, preferably a Na 2 SO 4 solution, or may consist of carbon powder mixed with concentrated Na 2 SO 4 .
  • the contacting layer 3 In order to ensure a back-up of the contacting layer material to the electrode, it is advantageous to press the contacting layer 3 with a constant pressure to the carrier layer 1. This can be done in different ways, for example by a tension on a rear wall, by means of springs, by hydraulic devices and the like. A Another possibility is to use the gas pressure of the electrolysis in the contact area.
  • Diamond electrodes designed and manufactured according to the invention can also be used as pipelar electrodes incorporated in an electrochemical cell.
  • electrochemical cells are used for various applications, for example, for water and wastewater treatment in industrial plants, for the purification of water in swimming pools or hot tubs and for the disinfection of drinking water.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

L'invention concerne un procédé de réalisation d'une électrode en diamant à partir de particules de diamant (2) de synthèse (dopées) et électriquement conductrices, ces particules étant insérées dans une couche support (1) en matériau électriquement non conducteur. Les particules de diamant (2) dopées sont placées en une couche entre deux feuilles formant la couche support (1), lesquelles sont reliées de manière fixe l'une à l'autre, les particules de diamant étant alors dégagées sur les deux faces de la couche support (1).
EP07727806.7A 2006-04-10 2007-04-04 Procédé de réalisation d'une électrode en diamant Active EP2004880B8 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AT0062006A AT503402B1 (de) 2006-04-10 2006-04-10 Verfahren zur herstellung einer diamantelektrode und diamantelektrode
PCT/EP2007/053337 WO2007116004A2 (fr) 2006-04-10 2007-04-04 Procédé de réalisation d'une électrode en diamant et électrode en diamant

Publications (3)

Publication Number Publication Date
EP2004880A2 true EP2004880A2 (fr) 2008-12-24
EP2004880B1 EP2004880B1 (fr) 2016-03-16
EP2004880B8 EP2004880B8 (fr) 2016-07-27

Family

ID=38495602

Family Applications (1)

Application Number Title Priority Date Filing Date
EP07727806.7A Active EP2004880B8 (fr) 2006-04-10 2007-04-04 Procédé de réalisation d'une électrode en diamant

Country Status (8)

Country Link
US (1) US8137515B2 (fr)
EP (1) EP2004880B8 (fr)
AT (1) AT503402B1 (fr)
DK (1) DK2004880T3 (fr)
ES (1) ES2573635T3 (fr)
PL (1) PL2004880T3 (fr)
PT (1) PT2004880E (fr)
WO (1) WO2007116004A2 (fr)

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US20100101010A1 (en) * 2008-10-24 2010-04-29 Watkins Manufacturing Corporation Chlorinator for portable spas
US8266736B2 (en) * 2009-07-16 2012-09-18 Watkins Manufacturing Corporation Drop-in chlorinator for portable spas
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AT511665A1 (de) 2011-06-30 2013-01-15 Pro Aqua Diamantelektroden Produktion Gmbh & Co Kg Tauchzelle zur elektrolytischen reinigung von wasser
AT511817B1 (de) * 2012-02-22 2013-03-15 Pro Aqua Diamantelektroden Produktion Gmbh & Co Kg Verfahren zur Herstellung einer Elektrode
AT511952B1 (de) * 2012-02-29 2013-04-15 Pro Aqua Diamantelektroden Produktion Gmbh & Co Kg Elektrolysezelle und Verfahren zu ihrer Herstellung
DE102013213981A1 (de) * 2013-07-17 2015-01-22 Rohde & Schwarz Gmbh & Co. Kg Spule für Schalteinrichtung mit hoher Hochfrequenzleistung
AT516720B1 (de) * 2015-05-18 2016-08-15 Pro Aqua Diamantelektroden Produktion Gmbh & Co Kg Verfahren zur Herstellung einer Elektrode
US10239772B2 (en) 2015-05-28 2019-03-26 Advanced Diamond Technologies, Inc. Recycling loop method for preparation of high concentration ozone
CN105624726A (zh) * 2015-12-30 2016-06-01 金刚宝石水高科技有限公司 用于电化学电池的电极
WO2018075920A1 (fr) 2016-10-20 2018-04-26 Advanced Diamond Technologies, Inc. Générateurs d'ozone, procédés de fabrication de générateurs d'ozone et procédés de génération d'ozone
CN109530896B (zh) * 2019-01-15 2021-08-13 青岛科技大学 一种通过阻焊法制作超硬磨料工具的新方法
DE102019134727A1 (de) * 2019-06-12 2020-12-17 Friedrich-Alexander-Universität Erlangen-Nürnberg Schweißelektrode und Verwendung der Schweißelektrode
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Also Published As

Publication number Publication date
AT503402A1 (de) 2007-10-15
US8137515B2 (en) 2012-03-20
WO2007116004A2 (fr) 2007-10-18
WO2007116004A3 (fr) 2008-03-13
PT2004880E (pt) 2016-06-07
EP2004880B1 (fr) 2016-03-16
ES2573635T3 (es) 2016-06-09
EP2004880B8 (fr) 2016-07-27
AT503402B1 (de) 2008-02-15
PL2004880T3 (pl) 2016-10-31
US20100170783A1 (en) 2010-07-08
DK2004880T3 (en) 2016-06-06

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